#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302759.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4302759
loop_
_publ_author_name
'Tori Z. Forbes'
'Slavi C. Sevov'
_publ_contact_author_address
;Department of Chemistry
University of Notre Dame
Notre Dame, IN 46556
;
_publ_contact_author_email       ssevov@nd.edu
_publ_contact_author_name        'Slavi C. Sevov'
_publ_section_title
;
Metal-Organic Frameworks with Direct Transition Metal-Sulfonate
Interactions and Charge-Assisted Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6873
_journal_page_last               6878
_journal_paper_doi               10.1021/ic9007922
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C22 H22 Mn N8 O6 S2'
_chemical_formula_sum            'C22 H22 Mn N8 O6 S2'
_chemical_formula_weight         613.56
_chemical_name_common            (Mn(Im)4)15NDS
_chemical_name_systematic
; 
 manganese tetraimidazole 1,5-napthalenedisulfonate hydrate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                60.31(3)
_cell_angle_beta                 86.79(3)
_cell_angle_gamma                74.06(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2113(16)
_cell_length_b                   9.802(2)
_cell_length_c                   9.862(2)
_cell_measurement_reflns_used    135
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      58
_cell_measurement_theta_min      2.5
_cell_volume                     660.0(3)
_computing_cell_refinement       'APEX II (Bruker, 2007)'
_computing_data_collection       'APEX II (Bruker, 2007)'
_computing_data_reduction        'APEX II (Bruker, 2007)'
_computing_molecular_graphics    'Crystalmaker 1.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      107(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'Bruker APEX II Diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20805
_diffrn_reflns_theta_full        37.87
_diffrn_reflns_theta_max         37.87
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.62790
_exptl_absorpt_correction_T_min  0.53349
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SADABS correction'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocky
_exptl_crystal_F_000             315
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.480
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0418P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                4676
_reflns_number_total             5998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9007922_si_002_4.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        660.0(2)
_cod_database_code               4302759
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.5000 0.5000 0.01332(7) Uani 1 2 d S . .
S1 S 0.24621(4) 0.91700(4) 0.31696(3) 0.01279(7) Uani 1 1 d . . .
O1 O 0.18793(13) 0.93939(12) 0.44827(10) 0.01876(19) Uani 1 1 d . . .
O2 O 0.32284(13) 0.74585(11) 0.36337(11) 0.0198(2) Uani 1 1 d . . .
O3 O 0.35611(13) 1.01844(12) 0.22648(11) 0.0208(2) Uani 1 1 d . . .
N1 N 0.31662(15) 0.40387(14) 0.43695(13) 0.0186(2) Uani 1 1 d . . .
N2 N 0.62540(15) 0.53961(14) 0.28156(12) 0.0186(2) Uani 1 1 d . . .
N3 N 0.19217(17) 0.24485(16) 0.41087(15) 0.0232(2) Uani 1 1 d D . .
N4 N 0.69427(18) 0.67695(17) 0.04196(14) 0.0276(3) Uani 1 1 d D . .
C1 C 0.06290(16) 0.98291(15) 0.18898(13) 0.0131(2) Uani 1 1 d . . .
C2 C 0.07609(16) 0.97343(15) 0.04822(12) 0.0128(2) Uani 1 1 d . . .
C3 C -0.09147(17) 1.04264(17) 0.22972(14) 0.0169(2) Uani 1 1 d D . .
C4 C -0.24085(18) 1.09331(19) 0.13360(15) 0.0210(3) Uani 1 1 d D . .
C5 C 0.23440(18) 0.91420(17) 0.00158(14) 0.0180(2) Uani 1 1 d D . .
C6 C 0.65289(19) 0.67841(18) 0.17522(17) 0.0234(3) Uani 1 1 d D . .
C7 C 0.6521(2) 0.44324(19) 0.21222(16) 0.0243(3) Uani 1 1 d D . .
C8 C 0.6938(2) 0.5276(2) 0.06368(17) 0.0299(3) Uani 1 1 d D . .
C9 C 0.3299(2) 0.25558(19) 0.4652(2) 0.0311(4) Uani 1 1 d D . .
C10 C 0.0856(3) 0.3961(3) 0.3382(4) 0.0724(10) Uani 1 1 d D . .
C11 C 0.1627(3) 0.4930(3) 0.3555(4) 0.0678(9) Uani 1 1 d D . .
H3 H -0.096(3) 1.048(3) 0.321(2) 0.050 Uiso 1 1 d D . .
H5 H 0.337(2) 0.880(3) 0.058(2) 0.050 Uiso 1 1 d D . .
H4 H -0.351(2) 1.133(3) 0.162(3) 0.050 Uiso 1 1 d D . .
H6 H 0.647(3) 0.772(2) 0.188(3) 0.050 Uiso 1 1 d D . .
H7 H 0.638(3) 0.337(2) 0.266(3) 0.050 Uiso 1 1 d D . .
H8 H 0.720(3) 0.499(3) -0.014(2) 0.050 Uiso 1 1 d D . .
H9 H 0.429(2) 0.167(2) 0.508(3) 0.050 Uiso 1 1 d D . .
H10 H -0.015(2) 0.430(3) 0.273(2) 0.050 Uiso 1 1 d D . .
H11 H 0.132(3) 0.607(2) 0.301(3) 0.050 Uiso 1 1 d D . .
H1 H 0.177(3) 0.154(2) 0.424(3) 0.050 Uiso 1 1 d D . .
H2 H 0.703(3) 0.763(2) -0.044(2) 0.050 Uiso 1 1 d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O2 180.0 2_666 . ?
O2 Mn1 N2 91.57(5) 2_666 . ?
O2 Mn1 N2 88.43(5) . . ?
O2 Mn1 N2 88.43(5) 2_666 2_666 ?
O2 Mn1 N2 91.57(5) . 2_666 ?
N2 Mn1 N2 180.0 . 2_666 ?
O2 Mn1 N1 92.20(5) 2_666 . ?
O2 Mn1 N1 87.80(5) . . ?
N2 Mn1 N1 89.68(5) . . ?
N2 Mn1 N1 90.32(5) 2_666 . ?
O2 Mn1 N1 87.80(5) 2_666 2_666 ?
O2 Mn1 N1 92.20(5) . 2_666 ?
N2 Mn1 N1 90.32(5) . 2_666 ?
N2 Mn1 N1 89.68(5) 2_666 2_666 ?
N1 Mn1 N1 180.0 . 2_666 ?
O1 S1 O2 112.61(7) . . ?
O1 S1 O3 112.66(6) . . ?
O2 S1 O3 112.03(7) . . ?
O1 S1 C1 106.84(6) . . ?
O2 S1 C1 105.56(7) . . ?
O3 S1 C1 106.55(6) . . ?
S1 O2 Mn1 155.72(7) . . ?
C9 N1 C11 103.97(14) . . ?
C9 N1 Mn1 130.28(11) . . ?
C11 N1 Mn1 125.74(11) . . ?
C6 N2 C7 105.50(12) . . ?
C6 N2 Mn1 125.03(11) . . ?
C7 N2 Mn1 127.86(9) . . ?
C9 N3 C10 106.32(15) . . ?
C9 N3 H1 124.8(16) . . ?
C10 N3 H1 128.8(16) . . ?
C6 N4 C8 107.58(12) . . ?
C6 N4 H2 123.2(16) . . ?
C8 N4 H2 128.5(16) . . ?
C3 C1 C2 121.28(12) . . ?
C3 C1 S1 117.70(9) . . ?
C2 C1 S1 121.02(10) . . ?
C5 C2 C2 119.20(13) . 2_575 ?
C5 C2 C1 122.66(12) . . ?
C2 C2 C1 118.14(14) 2_575 . ?
C1 C3 C4 119.79(11) . . ?
C1 C3 H3 119.5(15) . . ?
C4 C3 H3 120.7(15) . . ?
C5 C4 C3 120.94(13) 2_575 . ?
C5 C4 H4 118.1(14) 2_575 . ?
C3 C4 H4 121.0(14) . . ?
C4 C5 C2 120.64(13) 2_575 . ?
C4 C5 H5 116.0(14) 2_575 . ?
C2 C5 H5 123.4(14) . . ?
N2 C6 N4 111.44(14) . . ?
N2 C6 H6 126.0(14) . . ?
N4 C6 H6 122.6(14) . . ?
C8 C7 N2 109.60(14) . . ?
C8 C7 H7 129.3(14) . . ?
N2 C7 H7 121.0(14) . . ?
C7 C8 N4 105.87(14) . . ?
C7 C8 H8 131.5(14) . . ?
N4 C8 H8 122.7(14) . . ?
N1 C9 N3 112.95(15) . . ?
N1 C9 H9 125.2(15) . . ?
N3 C9 H9 121.4(15) . . ?
N3 C10 C11 106.57(18) . . ?
N3 C10 H10 125.5(15) . . ?
C11 C10 H10 127.1(15) . . ?
N1 C11 C10 110.15(17) . . ?
N1 C11 H11 120.9(16) . . ?
C10 C11 H11 127.4(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O2 2.1947(15) 2_666 ?
Mn1 O2 2.1947(15) . ?
Mn1 N2 2.2348(13) . ?
Mn1 N2 2.2348(13) 2_666 ?
Mn1 N1 2.2375(12) . ?
Mn1 N1 2.2375(12) 2_666 ?
S1 O1 1.4521(10) . ?
S1 O2 1.4531(11) . ?
S1 O3 1.4571(11) . ?
S1 C1 1.7739(14) . ?
N1 C9 1.3106(19) . ?
N1 C11 1.348(2) . ?
N2 C6 1.3155(19) . ?
N2 C7 1.3846(19) . ?
N3 C9 1.329(2) . ?
N3 C10 1.335(3) . ?
N3 H1 0.879(15) . ?
N4 C6 1.345(2) . ?
N4 C8 1.372(2) . ?
N4 H2 0.864(16) . ?
C1 C3 1.3709(19) . ?
C1 C2 1.4328(16) . ?
C2 C5 1.4218(18) . ?
C2 C2 1.422(2) 2_575 ?
C3 C4 1.407(2) . ?
C3 H3 0.926(15) . ?
C4 C5 1.3685(18) 2_575 ?
C4 H4 0.965(15) . ?
C5 C4 1.3685(18) 2_575 ?
C5 H5 0.919(16) . ?
C6 H6 0.975(16) . ?
C7 C8 1.359(2) . ?
C7 H7 0.940(16) . ?
C8 H8 0.938(15) . ?
C9 H9 0.940(16) . ?
C10 C11 1.355(3) . ?
C10 H10 0.950(16) . ?
C11 H11 0.934(16) . ?
